阅读说明：本技术 一种以β-环糊精包合白术药材中苍术酮成分的炮制方法 (A processing method of beta-cyclodextrin inclusion atractylone in Atractylodis rhizoma medicinal material ) 是由 张兆佳 梁云飞 蒙永明 蒙思宇 于 2020-12-01 设计创作，主要内容包括：本发明涉及医药技术领域,具体涉及一种以β-环糊精包合白术药材中苍术酮成分的炮制方法。该方法包括如下步骤：1)取白术药材,加入1～3倍量质量分数为33.3％～66.6％的β-环糊精-水共混物,搅拌均匀；2)对药材-β-环糊精-水的混合物进行45～95℃加热1～5h处理,加热过程中及时补充蒸发损耗的水；3)取出药材,40～80℃干燥3～9h。本方法用β-环糊精包合白术药材中苍术酮成分,将苍术酮从白术药材油室组织分离并进行保护,可有效避免粉碎过程中因油室组织被破坏而苍术酮严重流失的情况发生,提升药材粉碎后应用于中药制剂过程中的稳定性,有利于药材的质量控制。(The invention relates to the technical field of medicines, in particular to a processing method for including atractylone in a bighead atractylodes rhizome medicinal material by beta-cyclodextrin. The method comprises the following steps: 1) taking a bighead atractylodes rhizome medicinal material, adding a beta-cyclodextrin-water blend with the mass fraction of 33.3% -66.6% in an amount which is 1-3 times that of the medicinal material, and uniformly stirring; 2) heating the mixture of the medicinal materials, beta-cyclodextrin and water at 45-95 ℃ for 1-5 h, and supplementing water lost by evaporation in time in the heating process; 3) taking out the medicinal materials, and drying at 40-80 ℃ for 3-9 h. The method uses beta-cyclodextrin to include the atractylone component in the white atractylodes rhizome medicinal material, separates and protects the atractylone from the oil chamber tissue of the white atractylodes rhizome medicinal material, can effectively avoid the situation that the atractylone is seriously lost because the oil chamber tissue is damaged in the crushing process, improves the stability of the medicinal material after being crushed and applied to the traditional Chinese medicine preparation process, and is beneficial to the quality control of the medicinal material.)

1. A processing method for including atractylone in a white atractylodes rhizome medicinal material by beta-cyclodextrin is characterized by comprising the following steps:

1) cutting Atractylodis rhizoma, adding beta-cyclodextrin-water blend, and stirring;

2) heating the mixture of the medicinal materials-beta-cyclodextrin-water at 45-95 ℃ for 1-5 h;

3) taking out the medicinal materials, and drying.

2. The processing method as claimed in claim 1, wherein the amount of the β -cyclodextrin-water blend added in step 1) is 1-3 times of that of the Atractylodis rhizoma.

3. The processing method as claimed in claim 1, wherein the mass of the beta-cyclodextrin-water blend in step 1) is 2 times that of the rhizoma atractylodis macrocephalae.

4. The processing method as claimed in claim 1, wherein the mass fraction of the beta-cyclodextrin-water blend in the step 1) is 33.3-66.6%.

5. The processing method as claimed in claim 1, wherein the mass fraction of the β -cyclodextrin-water blend in step 1) is 45.0-55.0%.

6. The preparation method according to claim 1, wherein the cut length of the rhizoma Atractylodis Macrocephalae in step 1) is 1-3 cm.

7. The processing method as claimed in claim 1, wherein the water lost by evaporation is replenished in time during the heating in step 2) to maintain the concentration of the initial β -cyclodextrin-water blend.

8. The processing method as claimed in claim 1, wherein the heating temperature is 55-65 ℃ and the heating time is 2.5-3.5 h.

9. The processing method as claimed in claim 1, wherein the drying temperature in the step 3) is 40-80 ℃ and the drying time is 3-9 h.

10. The processing method as claimed in claim 1, wherein the drying temperature in the step 3) is 60-70 ℃, and the drying time is 4.5-6.5 h.

Technical Field

The invention relates to the technical field of medicines, in particular to a processing method for including atractylone in a bighead atractylodes rhizome medicinal material by beta-cyclodextrin.

Background

Common processing methods of the rhizoma atractylodis macrocephalae include a stir-frying method, a soil preparation method and a bran stir-frying method, which all belong to fire processing. The fire treatment of the atractylodes macrocephala koidz can achieve the purposes of reducing dryness and moderating drug property, but has obvious defects, and the high-temperature treatment can directly influence the quality stability of the heat-sensitive active ingredients of the atractylodes macrocephala koidz, such as atractylone. Atractylone can promote gastrointestinal peristalsis, can be converted into atractylenolide components through oxidation, plays an anti-tumor role by inducing apoptosis and inhibiting proliferation, and plays an anti-inflammatory role by inhibiting generation of cytokines mediating inflammatory reaction, regulating immunity and the like.

The volatile component atractylone contained in the bighead atractylodes rhizome is used as a main spot identified by thin-layer chromatography, and the higher the content of the atractylone, the larger the spot is, and the better the quality of the medicinal material is. Atractylone mainly exists in an oil chamber tissue of a medicinal material of the largehead atractylodes rhizome, is relatively unstable in property, is very volatile, and is easily decomposed by heat and light. The medicinal materials are crushed and applied to the Chinese medicinal preparation, the oil chamber tissue is damaged, and the atractylone is more easily volatilized and lost. Therefore, the fire-making method is not favorable for improving the quality stability of the rhizoma atractylodis macrocephalae in the preparation process.

At present, in order to avoid losing volatile oil components of the bighead atractylodes rhizome, beta-cyclodextrin is used for clathration of extracted volatile oil, for example, Kuliang and the like published in 'process research of volatile oil beta-cyclodextrin inclusion compound of bighead atractylodes rhizome'. However, no report is found on the method for avoiding the loss of volatile component atractylone in the processing process of the medicinal material of the largehead atractylodes rhizome.

Therefore, a processing method for improving the quality stability of the rhizoma atractylodis macrocephalae and performing inclusion protection on the atractylone in the rhizoma atractylodis macrocephalae is needed.

Disclosure of Invention

The invention aims to provide a processing method for including atractylone in a white atractylodes rhizome medicinal material by beta-cyclodextrin.

The technical scheme of the invention is as follows: a processing method for including atractylone in a white atractylodes rhizome medicinal material by beta-cyclodextrin comprises the following steps:

1) cutting Atractylodis rhizoma, adding beta-cyclodextrin-water blend, and stirring;

2) heating the mixture of the medicinal materials-beta-cyclodextrin-water at 45-95 ℃ for 1-5 h;

3) taking out the medicinal materials, and drying.

In the step 1), the addition amount of the beta-cyclodextrin-water blend is 1-3 times of that of the medicinal material of the largehead atractylodes rhizome.

The mass of the beta-cyclodextrin-water blend in the step 1) is 2 times that of the medicinal material of the largehead atractylodes rhizome.

The mass fraction of the beta-cyclodextrin-water blend in the step 1) is 33.3-66.6%.

Preferably, the mass fraction of the beta-cyclodextrin-water blend in the step 1) is 45.0-55.0%.

The length of cut rhizoma atractylodis macrocephalae in the step 1) is 1-3 cm.

Supplementing water lost by evaporation in time in the heating process in the step 2), and maintaining the concentration of the initial beta-cyclodextrin-water blend.

Preferably, the heating temperature is 55-65 ℃, and the heating time is 2.5-3.5 h.

In the step 3), the drying temperature is 40-80 ℃, and the drying time is 3-9 h.

Preferably, the drying temperature in the step 3) is 60-70 ℃, and the drying time is 4.5-6.5 h.

Compared with the prior art, the invention has the following beneficial effects:

a comparison graph of thin-layer spots of the processed rhizoma atractylodis macrocephalae and the unprocessed rhizoma atractylodis macrocephalae after high-temperature test for 0-31 days shows that the thin-layer identification characteristic spots of the unprocessed rhizoma atractylodis macrocephalae are gradually reduced, gradually disappear after 14 days, and completely disappear after 31 days, while the thin-layer characteristic spots of the rhizoma atractylodis macrocephalae processed by the method of the invention have no obvious change after 0-31 days. The beta-cyclodextrin is proved to be successfully included into the atractylone component, and the quality stability of the medicinal material is obviously improved. Therefore, the atractylone is separated from the oil chamber tissue of the bighead atractylodes rhizome medicinal material and protected, so that the situation that the atractylone is seriously lost due to the fact that the oil chamber tissue is damaged in the crushing process can be effectively avoided, the stability of the medicinal material after being crushed and applied to the traditional Chinese medicine preparation process is improved, and the quality control of the medicinal material is facilitated.

Drawings

FIG. 1: is a comparison graph of thin-layer spots after 9 days of high temperature test in experimental example 1, wherein the left part is the Atractylodis rhizoma processed by the method of example 2, and the right part is the untreated Atractylodis rhizoma.

FIG. 2: is a comparison graph of thin-layer spots after 14 days of high temperature test in experimental example 1, wherein the left part is the Atractylodis rhizoma processed by the method in example 2, and the right part is the untreated Atractylodis rhizoma.

FIG. 3: is a comparison graph of thin-layer spots after 31 days of high temperature test in experimental example 1, wherein the left part is the Atractylodis rhizoma processed by the method in example 2, and the right part is the untreated Atractylodis rhizoma.

Detailed Description

The following examples are further illustrative, but the present invention is not limited to these examples.

Example 1

1) Cutting a clean bighead atractylodes rhizome into 1-3 cm, adding a 1-time beta-cyclodextrin-water blend with the mass fraction of 33.3%, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water for 1h at 45 ℃, and supplementing water lost by evaporation in time in the heating process;

3) and (3) after the heating and inclusion are finished, taking out the medicinal materials in time, drying for 3h at the temperature of 40 ℃, and finishing the processing process.

Example 2

1) Cutting a clean bighead atractylodes rhizome into 1-3 cm, adding 2 times of a beta-cyclodextrin-water blend with the mass fraction of 50.0%, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water for 3h at 60 ℃, and supplementing water lost by evaporation in time in the heating process;

3) and (3) after the heating and inclusion are finished, taking out the medicinal materials in time, drying for 5 hours at the temperature of 65 ℃, and finishing the processing process.

Example 3

1) Cutting a clean bighead atractylodes rhizome into 1-3 cm, adding 3 times of a 66.6 mass percent beta-cyclodextrin-water blend, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water at 95 ℃ for 5h, and supplementing water lost by evaporation in time in the heating process;

3) and (3) after the heating and inclusion are finished, taking out the medicinal materials in time, drying for 9 hours at the temperature of 80 ℃, and finishing the processing process.

Example 4

1) Cutting a clean bighead atractylodes rhizome medicinal material into 1-3 cm, adding 2 times of a 45.0 mass percent beta-cyclodextrin-water blend, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal material-beta-cyclodextrin-water for 2.5h at 55 ℃, and supplementing water lost by evaporation in time in the heating process;

3) after the heating and clathration are finished, the medicinal materials are taken out in time and dried for 4.5h at the temperature of 60 ℃, and the processing process is finished.

Example 5

1) Cutting a clean bighead atractylodes rhizome into 1-3 cm, adding 3 times of a beta-cyclodextrin-water blend with the mass fraction of 55.0%, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water at 65 ℃ for 3.5h, and supplementing water lost by evaporation in time in the heating process;

3) after the heating and clathration are finished, the medicinal materials are timely taken out, dried for 6.5h at 70 ℃, and the processing process is finished.

Example 6

1) Cutting a clean bighead atractylodes rhizome medicinal material into 1-3 cm, adding 3 times of a beta-cyclodextrin-water blend with the mass fraction of 40.0%, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water for 4.0h at 50 ℃, and supplementing water lost by evaporation in time in the heating process;

3) after the heating and clathration are finished, the medicinal materials are taken out in time and dried for 6.0h at the temperature of 55 ℃, and the processing process is finished.

Example 7

1) Cutting a clean bighead atractylodes rhizome into 1-3 cm, adding 2 times of 60.0 mass percent beta-cyclodextrin-water blend, and uniformly stirring;

2) under normal pressure, heating the mixture of the medicinal materials-beta-cyclodextrin-water at 80 ℃ for 3.0h, and supplementing water lost by evaporation in time in the heating process;

3) after the heating and clathration are finished, the medicinal materials are timely taken out, dried for 4.0h at the temperature of 65 ℃, and the processing process is finished.

Experimental example 1

1. Purpose of the experiment: the stability of the quality of the processed Atractylodis rhizoma material of example 2 was compared with that of the untreated Atractylodis rhizoma material.

2. The experimental steps are as follows:

(1) the rhizoma atractylodis macrocephalae processed by the method and the unprocessed rhizoma atractylodis macrocephalae are subjected to a high-temperature test (T is 60 ℃, RH is 65%) at the same time, after the high-temperature test for 0-31 days, 0.5g of the rhizoma atractylodis macrocephalae and the unprocessed rhizoma atractylodis macrocephalae are respectively weighed, crushed and placed in a 50ml conical flask, 20ml of ethyl ether is added, the mixture is placed in a 45 ℃ water bath for low-temperature reflux for 1h, taken out, cooled and filtered, and the filtrate is concentrated to 1ml to be used as a test solution.

(2) Respectively taking 1 mu l of each of two test sample solutions, respectively dropping the two test sample solutions on the same silica gel G thin layer plate, taking petroleum ether (boiling range is 60-90 ℃) and dichloromethane (10:0.2) as a developing agent, developing, airing, spraying a 10% sulfuric acid ethanol solution of newly prepared 5% p-dimethylaminobenzaldehyde, and comparing the sizes of spots with the same color on corresponding positions of the two different test sample solutions.

3. The experimental results are as follows:

the results are shown in fig. 1-3, and it can be seen that the thin-layer characteristic spots of the untreated rhizoma atractylodis macrocephalae are gradually reduced, gradually disappear after 14 days, and completely disappear after 31 days, while the thin-layer characteristic spots of the rhizoma atractylodis macrocephalae processed by the method of the invention have no obvious change after 0-31 days. The beta-cyclodextrin is proved to be successfully included into the atractylone component, and the quality stability of the medicinal material is obviously improved. Therefore, the atractylone is separated from the oil chamber tissue of the bighead atractylodes rhizome medicinal material and protected, so that the situation that the atractylone is seriously lost due to the fact that the oil chamber tissue is damaged in the crushing process can be effectively avoided, the stability of the medicinal material after being crushed and applied to the traditional Chinese medicine preparation process is improved, and the quality control of the medicinal material is facilitated.